CHAPTER I

INTRODUCTION

Background of the Study

Activated carbon is a form of carbon that has been processed to create pores,

resulting in an increased surface area. Activated carbon is widely used for the treatment

of water and wastewater. This is an amorphous form of carbon with a large surface area.

It is mainly produced in laboratory using muffle furnace. The application of activated

carbon covers a wide spectrum of systems such as air purification, water and wastewater

treatments, and is also used in food, beverage, pharmaceutical and chemical industries.

Almost any carbonaceous material of animal, vegetable or mineral origin can be converted

into activated carbon if properly treated. Active carbons are produced from fossil coal or

various organic raw materials. Generally, good quality adsorbents can be obtained from

agricultural refuse.

Producing this kind of material exists in two forms: the carbonization of

carbonaceous raw material at temperature above 500˚C and the activation of the

carbonized product. Thus, all carbonaceous materials can be converted into activated

carbon, although the properties of the final product will be different, depending on the

nature of the raw material used, the nature of the activating agent, and the conditions of

the carbonization and activation processes.

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 However, the commercialized activated carbon is made in industrial furnaces like

the muffle furnace which is clearly more expensive which trigger the production cost of

the activated carbon to be expensive for the consumers that wants to avail it.

This study will develop and design an improvised furnace which will be capable of

converting waste material into Activated Carbon. In this way, there will be a cheaper

source of activated carbon in the market available to the local consumers. This would

also identify if the chosen waste materials are a potential source of carbon.

Statement of the Problem

The efficiency of the activated carbon in various application is compromised by its

expensive commercial price. Hence, this study will design, fabricate, and develop an

improvised furnace that will respond to the needs of the local consumers for a more

accessible and affordable source of activated carbon.

Statement of Objectives

This study aims to produce Activated carbon from waste materials using an

improvised furnace.

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 This study specifically aims to:

1. Design and construct an improvised furnace that is capable of converting

waste materials to Activated Carbon.

2. Identify if Calamansi peel is a potential source of carbon.

Significance of the Study:

This study will benefit the following:

Environment. The outcome of the study will reduce the proliferating number of

organic waste which contributes to pollution.

Community. The outcome of the study will create an alternative way of converting

waste materials into activated carbon which will provide them a cheaper source of it.

Agricultural Industries. The outcome of the study can provide the industries an

idea of how to carbonize any material within a small span of space which is a more

efficient.

Future researchers. The outcome of the study can help them explore what other

waste materials can they convert into activated carbon and this will give them an idea of

what problem could they solve with this process.

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Scope and Limitations

The researchers will conduct the experiment for a duration of 1 month starting

from the month of February up to March of 2019. The testing of the research will be

conducted within Central Philippine University, while the materials will be gathered here

in Iloilo City.

The study aimed to develop an improvised furnace that is capable of converting

waste materials to activated carbon. The study limits its coverage only in the production

of improvised foundry and does not cover testing of the strength and durability (e.g.

tensile strength) of materials that will be used in the making of improvised furnace.

In the product testing and experimentation, the product made by the improvised

furnace will be tested at the chemical laboratory of Central Philippine University to see

whether it is an activated carbon or not.

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 CHAPTER II

REVIEW OF RELATED LITERATURE

Activated carbon

Activated carbon was first produced on an industrial scale at the beginning of the

twentieth century, and major developments then took place in Europe. The Swedish

chemist von Ostreijko obtained two patents, in 1900 and 1901, covering the basic

concepts of chemical and physical activation of carbon with metal chlorides and carbon

dioxide and steam, respectively (Sontheimer, 1988). In 1909, a plant named ‘Chemische

Werke’ was built to manufacture, for the first time on a commercial scale, the powdered

activated carbon Eponits and Norits (Dabrowski, 1998). There were similar developments

in the United States at the same time. The first activated carbon was produced from black

ash, a waste product of soda production, for decolorizing liquids (Hassler, 1963).

The first commercial production of activated carbon in the United States took place

in 1913 (Hendricks, 2006). Almost any organic matter with a large percentage of carbon

could theoretically be activated to enhance its adsorption capacity. In practice, however,

the best sources of activated carbon should have a high carbon content, a long storage

life, are hard enough to maintain their properties under usage conditions, are obtainable

at a low cost, and capable of producing a high-quality activated product when processed

(Bansal et al., 1988).

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 Activated carbon is a highly porous carbonaceous material engineered for different

applications. It is substance derived from organic material (usually woody, fibrous stuff).

The useful thing about activated carbon is that it can filter out contaminants from both

water and air, which makes it an important substance in filtration system. This internal

porosity created is manifested by the extensive area generated on the surface of

thmaterial. Common applications of activated carbon include the removal of organic and

inorganic contaminants from liquid and gas streams, the separation of gases, and the

support for heterogeneous catalysts, etc. One of the most widely known applications is

the purification of water and beverages, due to its particular affinity to organic compounds.

Liquid applications include the removal of dissolved organics from waste water, along

with color, odor and undesired flavors from drinking water. The filtration of specific

compounds from gas effluents,such as mercury, is another main application of activated

carbon. It is often used in mercury scrubbing by impregnating the carbon material with

chloride. Mercury scrubbing is utilized in many coal power stations and incinerators and

natural gas wellheads. Food product decolorizing, such as sugars and molasses, is

another frequent use of activated carbon. The raw concentrated liquor is percolated

through powder or granular AC and colored bodies and some mineral ash is removed

from the solution. Molasses number is a typical test performed to compare the amount of

colored bodies removed from the solution of different adsorbents, and are compared to a

standard carbon. The good de-colorization materials have high surface area but most

importantly, favorable relation of micro and macro pore which are vital for the removing

of polydisperse colorants.

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 Activated carbon is broadly defined to include a wide range of amorphous carbon

based materials prepared in such a way that exhibit a high degree of porosity and an

extended surface area. For many centuries the activated carbon was used in the form of

carbonized wood. The earliest known use of carbon in the form of wood chars by the

Egyptians and Sumerians was in 3750 BC for the reduction of ores in the manufacturing

of bronze, domestic smokeless fuel and medicinal application. In 1500 BC, Egyptian

papyri was used as adsorbent for odorous vapours from putrefying wounds and from

within the abdominal tract. The wrecks of Phoenician trading ships suggest that drinking

water was stored in charred wooden barrels. This practice was certainly still in use in the

18th century for extending the use of potable water on long sea voyages. The ancient

Hindus in India of the same period (450 B.C) used sand and charcoal filters for purifying

drinking water. In 157 AD Claudius Galvanometer referred the use of carbons of both

vegetable and animal origin for the treatment of a wide range of diseases. The specific

adsorptive capacity of charcoal was recognized by Scheele at 1773 AD, who measured

the volumes of gases that could be adsorbed by carbons derived from different sources.

In 1785, Lowitz reviewed the abilities of charcoals to adsorb odors and vapours from a

range of organic chemicals. He also studied the effectiveness of charcoal in decolourizing

tartaric acid. In 1794 wood charcoal was used to decolourize the sugar cane syrups. In

1811, Figuier evaluated the decolourizing capacity of bone char and wood char and

during 1815, most of the sugar refining industry had switched to the use of granulated

bone char as a decolorant. Joseph de Cavaillon patented a method for regenerating used

bone chars in 1817. Bussy (1822) demonstrated that the decolorizing properties of

carbons were inherent to the source material and also depended on the thermal

7
processing and the particle size of the finished product. Kayser (1881) firstused the term

adsorption to describe the uptake of gases by carbons. The basis for the industrial

production of activated carbon from coal was established in 1900 in order to replace the

bone char in the sugar refining process.

The first powdered commercial activated carbon, eponite was produced in Europe in

1909. During the First World War (1914), steam activation of coconut shell and almond

shell char was developed in the United States for use in gas masks. It has been used

subsequently for water treatment, solvent recovery and air purification. This type of

activated carbon mainly contains fine pore structures suited for gas phase adsorption

applications. In Czechoslovakia two varieties of pelletized carbons were produced (1935–

1940) from sawdust by zinc chloride activation, for the recovery of volatile solvents and

for the removal of benzene from town gas. Nowadays the zinc chloride process of

chemical activation has been largely superseded by the use of phosphoric acid. Barrer &

Breck (1956) invented the method of zeolite synthesis. In that year the North-American

Linde Company started production of synthetic zeolites on a commercial scale

(Dabrowski 2001, Ferhan & Ozgur 2011, John 1974). The use of carbon molecular sieves

in gas separation, in particular oxygen and nitrogen, has grown steadily in the past years

(Sircar et al 1996). Activated carbons are useful adsorbents due to their porous

structures, the presence of various oxygenated functional surface groups depending on

the precursor’s nature and the procedures used in their preparation, and thus activated

carbons show differences in their adsorptive behavior. To produce these carbons,

chemical, physical and mixture of both as activating agents are used and a number of

activation procedures have been reported in the literature (Bansal et al 1988) using the

8
above said activating agents. In general it can be classified either as single stage or two-

stage process.

Activated carbon also called activated charcoal, is a form of carbon that has been

processed with oxygen to create millions of tiny pores between the carbon atoms.

Commercial activated carbons have internal surface area ranging from 500 to 1500 m2

/g. Activated carbon can be prepared from feed stock with high carbon and low inorganic

content. The most common feed stocks used for the production of activated carbon are

wood, coconut shell, bituminous coal, peat etc. The chars obtained from them could be

activated easily to produce reasonably high quality activated carbons. During the

activation process, the unique internal pore structure is created, which provides the

activated carbon its outstanding adsorptive properties.

Methylene Blue Number

The methylene blue number is defined as the maximum amount of dye adsorbed on 1.0

g of adsorbent. Adsorption experiments of the molecules of methylene blue are easy and

habitually done to characterize activated carbons with the purpose of obtaining information on

the adsorption capacity of the materials. According to the dimensions of the methylene blue

molecule, it is mainly adsorbed in mesopores, however, a small portion is also found in larger

micropore. (Shrestha, 2016)

Methylene number is a parameter of active carbon (AC) which gives opportunity to indicate

de-coloring properties of AC (sorption properties in solutions). Methylene blue (CI 52015) is a

heterocyclic aromatic chemical compound with the molecular formula C16H18N3SCl. It has many

9
uses in a range of different fields, such as biology and chemistry. At room temperature it appears

as a solid, odorless, dark green powder that yields a blue solution when dissolved in water. The

hydrated form has 3 molecules of water per molecule of methylene blue.

Calamansi Peel

Calamondin (Citrofortunella microcarpa) fruits or locally known as “Kalamansi” is widely

cultivated in Philippines and is used as a condiment almost in every famous dish made in the

Philippines. Only the pulp were squeezed and is needed, the peels are just thrown away. It

belongs to the family Rutaceae. It is an intergenetic hybrid between a member of Citrus reticulata

or “tangerine” and “kumquat” or Fortunella japonica. (Morte, 2017)

The Calamansi is well known as a medicinal plant, but it can be more flexible if we know how to

make it work and we can be more creative on how we present it.

Furnace

Carbonizing furnace is one of the most important equipment in making

charcoal. Its importance in the production of charcoal is undoubted. The production

personnel should pay attention to the regulation in the use of carbonizing furnace and

carefully grasp the production process to ensure the safety and quality of charcoal

production line. (Chou, 2014)

In the Philippines, Traditional charcoal production is an acquired skill. The most

critical factor in the efficient conversion of wood to charcoal is the careful operation of

10
the kiln. Wood must be dried and carefully stacked to allow an even flow of air through

the kiln and sufficient time for reactions to take place. If kilns are not operated correctly,

yields can be half the optimum level.

Much charcoal for domestic consumption in developing countries is produced in pit

kilns (holes dug in the ground), or in mound kilns (piles of wood stacked on the ground

and covered with soil), by farmers and landless laborers. Yields (weight of

charcoal/weight of wood) from pits vary from less than 10 per cent to over 25 per cent.

Charcoal is important in terms of energy and economies within most third-world

countries. The production of charcoal employs a considerable number of people in rural

areas. However, charcoal users as the group are most strongly exposed to carbon

monoxide (CO), followed by wood users. Charcoal use also results in high volumes of

carbon dioxide (CO2) emissions contributing to global warming.

Increasing end-use efficiency requires the promotion of improved stoves.

Traditional stoves are normally made by the informal sector; models with higher heat

transfer efficiencies should be developed in collaboration with end-users and stove

producers, and manufactured by the private sector.

Inefficiencies inherent to the production and use of charcoal, rapid urbanization

and the preference of urban dwellers for charcoal place a heavy strain on local wood

resources. Financial loans helped people cover the costs of converting as cost was seen

as the dominant constraint. Introducing LPG or Kerosene reduces the particle pollutants,

11
which result in improved long-term health benefits when compared with traditional fuel

wood or charcoal use for cooking.

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 CHAPTER III

METHODOLOGY

Collection of material

Conceptualization and Fabrication of the Furnace

Preparation of Calamansi peelings

Preparation of fuels

Production and Activation of Carbon

Collection and Analyzation of Data

Figure 1. Flowchart of Methods

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Collection of materials

The researchers will collect the materials needed to conduct this study. For the furnace,

the researchers will need an empty gas cylinder, plaster, metal bars, angle bars, and metal

tubings. Coal acted as the fuel of the study and the air pump was used to constantly aid the coal

in its temperature. The researcher also collected a sufficient amount of Calamansi peelings. For

the laboratory testing, the researchers borrowed 21 beakers, 21 Erlen Meyer flasks, and 21

filtration setup which includes funnels, Whatman 41 filter papers, iron stands, and iron rings. The

reseachers provided their own chemicals such as 2.5g of Methylene blue and 50mg Zinc Chloride.

Conceptualization and Fabrication of the Furnace

The researchers designed the furnace in

accordance with the result they want to get. The lid of

the furnace was given a hole in the center measuring

1.4 inches in radius to serve as the vent line. The lid

itself has a radius of 6 inches to fit it with the base of

the furnace.

Figure 2. Design of the

furnace with dimension

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 The insulation in the base of the furnace was 2 inches thick to prevent the heat from

coming out. This will also ensure that the base of the furnace is sturdy enough to withstand an

environment with high heat. The researchers also placed a feet that

measures 8 inches to stabilize it and prevent it from falling.

The crucible used measures 5 ½ inches in height and 2

inches in radius. This measurements were made by the researchers

to secure that the crucible fits the furnace.

Figure 3. Design of the
crucible with dimension

Preparation of Calamansi peels

The Researcher gathered the test subject in the market and in food stalls wherein the

peelings of the Calamansi is put directly to waste. After gathering the peelings, the researchers

sun dried the Calamansi for four days.

Preparation of the fuel

The researchers prepared an air pump that was connected to the gas cylinder by a rubber

tubing. The coal will occupy of the fuel section for it will be the key fuel in sustaining the intended

temperature inside the furnace. The researchers also added coal every one hour in the duration

of the experiment.

15
Production and Activation of Carbon

The researchers prepared the Calamansi peel where it was palced inside the crucible then,

it was subjected to the furnace. The Calamansi peels were carbonized using the improvised

furnace for about six to seven hours and was set for another 6 hours. The sample as then

pulverized until reached the intended texture.

Figure 4. Mixture of pulverized Figure 5. Washing and filtering

carbon and the solution of Zinc the activated carbon
Chloride

Figure 6. Removal of moisture

of activated carbon

The researcher also prepared a zinc chloride solution with 50 mg of zinc chloride mixed

with 150 mL of distilled water. The carbon and the zinc chloride solution was combined until it

achieved a past-like texture. The mixture was set for 24 hours to provide a complete activation

of the carbon. After its activation, the carbon was rinsed in distilled water and was filtered using

a coffee filter. The filtrant was dried in an oven for 30 minutes in 225°F.

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Application of Activated Carbon

The researchers tested the effectivity of the generated activated carbon by its Methylene

blue number. The researchers prepared a 1000 ppm base concentration as a source of the

solution that was used to be subjected to the activated carbon. They will prepare seven different

concentration with one replicate and one control variable with the use of commercial activated

carbon.

Figure 7. Combining the Activated

carbon and the Methylene Blue Solution

The researchers prepared 7 different concentration to test the absorbance of the activated

carbon from Calamansi Peelings and the commercial one.

After preparing the concentration, the researchers added 20 mL of each concentration in

a separate container with 0.1g of activated carbon and it was then left to set for 15 hours. This

was filtered after the addition of activated carbon.

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Collection and Analyzation of the data

After conduct of the study, the researchers will gather significant data for this study. The

ash of the waste materials will be tested for its activated carbon content. The absorbance level

of each filtrate was subjected to the UV-Vis spectrophotometer. The gathered data was then

compared to the base concentrations’ absorbance level and compare it to the result of the control

variable to see if there is a significant difference between the results.

Figure 8. Filtered sample of the Activated

Carbon and Methylene blue mixture

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 CHAPTER IV

RESULTS AND DISCUSSION

This chapter deals with the results of the activated carbon produced and its

implication to the community.

BASE CONCENTRATION ABSORBANCE

10 0.8312

25 1.328

50 2.36

100 2.486

250 2.486

500 2.486

1000 2.486

Table 1. Absorbance level of the original concentrations of Methylene blue solution

The table shows that portions of activated carbon were prepared from Calamansi

peels and the resultant carbons were characterized by methylene blue with different

concentrations with three replicate each.

20 ml of the different concentration was added in each container which contains

0.1g of activated carbon, both the experimental and the commercial one, and was then

left to set for 15 hours.

19
 TRIALS

SETUP A B C

1 0.030 Abs. 0.030 Abs. 0.027 Abs.

2 0.405 Abs. 0.268 Abs. 0.042 Abs.

3 1.282 Abs. 1.409 Abs. 0.051 Abs.

4 2.419 Abs. 2.419 Abs. 0.064 Abs.

5 2.500 Abs. 2.500 Abs. 0.059 Abs.

6 2.500 Abs. 2.500 Abs. 0.086 Abs.

7 2.500 Abs. 2.500 Abs. 0.103 Abs.

Table 2. The absorbance level of the sample subjected to UV-Vis Spectrophotometer

Table 2 shows the three replications of each concentration, two replicates for the

Activated carbon made from Calamansi peel and another one for the commercialized

activated carbon which served as the control variable of the study. This shows that

there is a significant difference between the Activated carbon made in the improvised

furnace from the Calamansi peels and the commercial one. It shows that the activated

carbon made from Calamansi peels has a comparable absorbance value with the

commercialized one.

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 CHAPTER V

CONCLUSION AND RECOMMENDATION

Conclusion

Based on the results obtained, the researchers came up with the following

conclusions:

1. The absorbance value of 0.1g of activated carbon made from calamansi

(citrofortunella microcarpa) peels in 10 ppm and 25 ppm are comparable with

the absorbance value of the commercial one.

2. The absorbance value of 0.1g of activated carbon made from calamansi peels in

50 ppm and 100 ppm have a huge compared to the commercial one.

3. The furnace designed by the reseachers is capable to carbonized waste

materials, specifically calamansi peelings in this study.

4. Calamansi peelings can be a potential source of carbon and is feasible in

converting it into activated carbon.

Recommendation

For the development of production of activated carbon, the researchers suggest

the following:

1. To use another waste material that have a significant effect on the environment

to be converted into activated carbon.

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2. To use another chemical process to test the effectivity of the activated carbon.

3. To use different ratio of materials in the fabrication of the base of the furnace.

4. To formulate a unique design of a furnace that can withstand high temperature

for a longer period of time.

22